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WO1989002481A1 - Procede et dispositif de traitement de boues d'hydroxyde - Google Patents

Procede et dispositif de traitement de boues d'hydroxyde Download PDF

Info

Publication number
WO1989002481A1
WO1989002481A1 PCT/EP1988/000799 EP8800799W WO8902481A1 WO 1989002481 A1 WO1989002481 A1 WO 1989002481A1 EP 8800799 W EP8800799 W EP 8800799W WO 8902481 A1 WO8902481 A1 WO 8902481A1
Authority
WO
WIPO (PCT)
Prior art keywords
copper
hydroxide
solution
nickel
container
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP1988/000799
Other languages
German (de)
English (en)
Inventor
Rolf Reuter
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Gut Gesellschaft fur Umweltschonende Technik Mbh
Original Assignee
Gut Gesellschaft fur Umweltschonende Technik Mbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Gut Gesellschaft fur Umweltschonende Technik Mbh filed Critical Gut Gesellschaft fur Umweltschonende Technik Mbh
Priority to FI892164A priority Critical patent/FI892164A0/fi
Priority to KR1019890700805A priority patent/KR890701781A/ko
Priority to AT88907682T priority patent/ATE78303T1/de
Priority to BR8807193A priority patent/BR8807193A/pt
Priority to DE8888907682T priority patent/DE3872870D1/de
Publication of WO1989002481A1 publication Critical patent/WO1989002481A1/fr
Priority to DK221289A priority patent/DK221289A/da
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/203—Iron or iron compound
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/06—Controlling or monitoring parameters in water treatment pH
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a method and an apparatus for processing hydroxide sludges.
  • hydroxide slurries occur primarily in electroplating processes and, because of their relatively high proportions of heavy metals such as chromium, iron, copper, nickel and possibly zinc, represent a considerable environmental problem.
  • the object of the present invention is to provide a method and a device which make it possible to process such hydroxide sludges, in particular hydroxide sludges which contain chromium, iron, copper, nickel and optionally zinc, in such a way that they are processed by them Hydroxide sludges have no or negligible environmental pollution.
  • this object is achieved in that, in the presence of zinc, the zinc hydroxide is dissolved from the sludge by alkali, and then the chromium hydroxide in the residue of the alkali treatment is oxidized to chromate in a weakly alkaline medium, that from the residue of the Oxidation or alkali treatment copper and nickel can be solved by acid treatment, that the residual sludge consisting essentially of iron hydroxide is separated from the solution containing copper and nickel, that copper oxide is precipitated from the solution containing copper and nickel, and that the precipitated copper oxide is separated from the nickel containing solution is separated.
  • the device of the invention for achieving the object is characterized by having a Be Schol lei ⁇ cardi reaction vessel provided, which is connected to a receiving vessel via a filter, a container with the Itemss ⁇ connected Reagensdosiervorrichtu ⁇ g, a circulation system with a circulating line 'containing a circulating pump and the Storage tank connects to the reaction tank, a discharge device that connects the filter with a storage tank for residual sludge contained in the aqueous iron hydroxide, and storage tanks each for zincate solution, chromate solution, nickel solution and copper solution, each on the input side via controlled valves with the storage tank and on the output side via controlled valves the circulation system or a further processing system can be connected.
  • the method and the apparatus erfindungsge ⁇ Permitted '' thus enable a full work-up of the Q Hydroxidschlammes under separation into its individual components.
  • the processing is carried out using procedural measures which - themselves do not cause any significant environmental pollution. It is achieved in this way that there is no need to deposit the hydroxide sludge.
  • a particular advantage is achieved in that the workup is carried out in a one-pot process and the solutions of the separated constituents are circulated. The result of this is that the solutions of the individual components can be enriched to such an extent that further processing with recovery of the valuable material is worthwhile.
  • the drawing shows schematically a device for processing hydroxide sludges.
  • the device described below represents a preferred exemplary embodiment which is used for the batchwise processing of hydroxide sludge. especially 1 of hydroxide sludge of the type obtained in electroplating processes is suitable.
  • the Aufailleungsvejrfahren can with equal effectiveness in a number hinterdenge- switched 'reaction containers are made, in which the individual working-up steps are carried out separately.
  • the device contains a reaction container 1 which is provided with a filling device 2 which is connected to the inlet side of the reaction container 1 via a controlled valve 3.
  • the reaction container 1 is further provided on the input side with a reagent metering device 4, the storage containers 4A, 4B and 4C of which are each connected to the reaction container 1 via controlled valves 5; the stirrer 6 of a conventional agitator extends into the interior of the reaction container 1.
  • a discharge device 8 of conventional design is connected to the filter 7, by means of which the filter residue is conveyed from the filter 7 into a collecting container 9.
  • the storage container 10 is connected to the input side of the reaction container 1 via a controlled valve 14 and a circulation system 11 comprising a circulation line 12 and a circulation pump 13.
  • the reservoir 10 is also connected via a controllable valve 15 to collecting tanks 16, 17, 18 and 19, which each hold the solutions of the separated components of the hydrogen oxide sludge.
  • the collection containers 16 to 19 are optionally on the output side via controlled valves 20 with further processing systems, for example electrolysis systems, which are not shown in detail.
  • gene, or a feed line 21 can be connected to the input side of the circulation pump 13 of the circulation system 11.
  • a conventional programmable control device 25 is provided, to which the controlled valves 3, 5, 14, 15 and 20, as well as the circulation pump 13, the discharge device 8 and a pH sensor 26 arranged in the interior of the reaction container 1 are connected and which controls the method described below according to a predetermined program sequence.
  • the plant described above for working up a chromium, iron, copper, nickel and optionally zinc-containing hydroxide sludge is operated as follows.
  • the reaction steps for separating zinc can be omitted if the hydroxide sludge does not contain zinc hydroxide.
  • Exercise is assumed that the collection containers contain 16 to 19 zincate solution, chromate solution or nickel solution or copper solution.
  • the first reservoir 4A contains aqueous alkali, e.g. B. sodium hydroxide solution
  • the second reservoir 4 B is an aqueous hydrogen peroxide solution
  • the third reservoir 4C is an aqueous acid, for example hydrochloric acid. If necessary, it can be provided between the individual separation steps that the respective residues are washed with water.
  • the circulation is ended after a predetermined reaction time.
  • the solution containing the chromate is filtered through the filter 7 into the storage container 10 and the filtrate is transferred from the storage container 10 into the collection container 16.
  • the residue from the alkali treatment in the reaction container 1 is then oxidized by removing chromate solution from the collecting container 16 and introducing it into the reaction container 1.
  • acid or alkali is then added, as a result of which a pH in the range from 8 to 11 is set in the reaction vessel 1.
  • a sufficient amount of hydrogen peroxide is metered in from the second storage container 4B.
  • the slurry is then stirred and at the same time the circulation system 11 is put into operation.
  • the sludge remaining in the reaction container is then slurried in acidic nickel solution from the collecting container 18, the pH being adjusted to a value in the range of 3.5 by adding acid from the third storage container 4C. .Under these conditions go copper and nickel in solution, while a residual sludge, which contains' substantially iron hydroxide remains.
  • the solution of copper and nickel obtained is filtered through the filter 7 into the storage container 10.
  • the residual sludge remaining on the filter 7 is discharged by means of the discharge device 8 and collected in the collecting container 9.
  • the residual sludge can be removed from this collecting container 9 and processed further, for example, to iron oxide.
  • the solution is then returned from the storage container 10 into the reaction container 1 and adjusted to a pH in the range from 4 to 6 by adding aqueous alkali from the first storage container 4A. Then hydrogen peroxide is added from the first storage container 4A, as a result of which this is in the solution contained copper is precipitated as copper oxide. After a predetermined period of time, the copper oxide is filtered off through the filter 7 and the solution containing nickel is transferred to the collecting container 18.
  • the copper oxide residue remaining on the filter 7 is dissolved in the acidic copper solution, which is removed from the collecting container 19 and optionally adjusted to the desired acidity with acid from the third storage container 4C.
  • the copper-containing solution is then returned to the collecting container 19.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Hydrology & Water Resources (AREA)
  • Mechanical Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Treatment Of Sludge (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Removal Of Specific Substances (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

On traite successivement des lots de boues d'hydroxyde avec divers agents chimiques dans un récipient de réaction, transformant ainsi par oxydation l'hydroxyde de chrome en chromate. On extrait l'hydroxyde de zinc à l'aide d'alcalis. L'hydroxyde de chrome dans le résidu du traitement alcalin est transformé en chromate par oxydation. On extrait du cuivre et du nickel à partir des résidus d'oxydation, avec des acides. La boue résiduelle restante contient essentiellement de l'hydroxyde de fer. L'oxyde de cuivre est précipité à partir de la solution, separé de la solution de nickel et finalement dissous dans l'acide. La séparation peut être effectuée dans un seul récipient et produit les constituants séparés de la boue d'hydroxyde sous une forme permettant leur récupération comme matières utiles.
PCT/EP1988/000799 1987-09-07 1988-09-02 Procede et dispositif de traitement de boues d'hydroxyde Ceased WO1989002481A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
FI892164A FI892164A0 (fi) 1987-09-07 1988-09-02 Foerfarande och anordning foer behandling av hydroxidsuspensioner.
KR1019890700805A KR890701781A (ko) 1987-09-07 1988-09-02 수산화물 슬라지를 정련하기 위한 방법과 장치
AT88907682T ATE78303T1 (de) 1987-09-07 1988-09-02 Verfahren und vorrichtung zur aufarbeitung von hydroxidschlaemmen.
BR8807193A BR8807193A (pt) 1987-09-07 1988-09-02 Processo e dispositivo para o preparo de lodos de hidroxido
DE8888907682T DE3872870D1 (de) 1987-09-07 1988-09-02 Verfahren und vorrichtung zur aufarbeitung von hydroxidschlaemmen.
DK221289A DK221289A (da) 1987-09-07 1989-05-05 Fremgangsmaade og anlaeg til oparbejdning af hydroxid-slam

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP3729913.1 1987-09-07
DE19873729913 DE3729913A1 (de) 1987-09-07 1987-09-07 Verfahren und vorrichtung zur aufarbeitung von hydroxidschlaemmen

Publications (1)

Publication Number Publication Date
WO1989002481A1 true WO1989002481A1 (fr) 1989-03-23

Family

ID=6335411

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1988/000799 Ceased WO1989002481A1 (fr) 1987-09-07 1988-09-02 Procede et dispositif de traitement de boues d'hydroxyde

Country Status (11)

Country Link
EP (1) EP0333796B1 (fr)
JP (1) JPH02501578A (fr)
KR (1) KR890701781A (fr)
AT (1) ATE78303T1 (fr)
AU (1) AU609191B2 (fr)
BR (1) BR8807193A (fr)
DE (2) DE3729913A1 (fr)
DK (1) DK221289A (fr)
ES (1) ES2008025A6 (fr)
FI (1) FI892164A0 (fr)
WO (1) WO1989002481A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6716403B2 (en) * 2000-11-14 2004-04-06 Japan Pionics Co., Ltd. Method of recovering a cleaning agent
CN103014337A (zh) * 2013-01-10 2013-04-03 北京矿冶研究总院 一种酸浸溶液中铜、铬、锌的分离方法

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20010110611A (ko) * 2000-06-07 2001-12-13 임수선 귀금속 분진 회수장치.
TWI671408B (zh) * 2014-12-25 2019-09-11 日商三菱綜合材料股份有限公司 脫銅黏泥（ｓｌｉｍｅ）所含之有價金屬的浸出方法
CN108048656A (zh) * 2017-11-13 2018-05-18 陕西省商南县东正化工有限责任公司 一种含铬铜镍的电镀废料的分离方法
CN114293015B (zh) * 2021-12-06 2023-05-09 生态环境部华南环境科学研究所 一种用于电镀污泥重金属提取回收的提取方法及其设备

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2023410A1 (de) * 1969-05-14 1970-11-19 M. 4 T. Chemicals Inc., New York City, N.Y. (V.St.A.) Verfahren zur Rückgewinnung von Nickel aus nickelhaltigen Schlämmen
US3816306A (en) * 1972-05-19 1974-06-11 C Roy Copper etchant effluent treatment
US4105743A (en) * 1976-06-15 1978-08-08 Mx-Processer Reinhardt & Co. Ab Selectively extracting copper, zinc, nickel from a mixture of metal hydroxides
US4162294A (en) * 1977-09-29 1979-07-24 Th. Goldschmidt Ag Process for working up nonferrous metal hydroxide sludge waste
FR2436821A1 (fr) * 1978-09-22 1980-04-18 Goldschmidt Ag Th Procede de traitement de residus de boues d'hydroxydes de metaux lourds non ferreux
US4318788A (en) * 1979-12-12 1982-03-09 Andco Environmental Processes, Inc. Chromate recovery process
US4465593A (en) * 1982-03-23 1984-08-14 Environmental Technology (U.S.), Inc. Recovery of metal from waste water by chemical precipitation
DE3308179A1 (de) * 1983-03-08 1984-11-29 Argentum Beck Und Gebhart Ohg Vorrichtung zum entgiften von oxidierbare organische und/oder anorganische substanzen enthaltende fluessigkeiten
US4579721A (en) * 1984-08-03 1986-04-01 Getty Oil Company Process for recovering metals from waste
US4680126A (en) * 1986-02-18 1987-07-14 Frankard James M Separation and recovery of reusable heavy metal hydroxides from metal finishing wastewaters

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4105243A (en) * 1971-03-12 1978-08-08 Daimler-Benz Aktiengesellschaft Outer body panel structure for vehicle bodies

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2023410A1 (de) * 1969-05-14 1970-11-19 M. 4 T. Chemicals Inc., New York City, N.Y. (V.St.A.) Verfahren zur Rückgewinnung von Nickel aus nickelhaltigen Schlämmen
US3816306A (en) * 1972-05-19 1974-06-11 C Roy Copper etchant effluent treatment
US4105743A (en) * 1976-06-15 1978-08-08 Mx-Processer Reinhardt & Co. Ab Selectively extracting copper, zinc, nickel from a mixture of metal hydroxides
US4162294A (en) * 1977-09-29 1979-07-24 Th. Goldschmidt Ag Process for working up nonferrous metal hydroxide sludge waste
FR2436821A1 (fr) * 1978-09-22 1980-04-18 Goldschmidt Ag Th Procede de traitement de residus de boues d'hydroxydes de metaux lourds non ferreux
US4318788A (en) * 1979-12-12 1982-03-09 Andco Environmental Processes, Inc. Chromate recovery process
US4465593A (en) * 1982-03-23 1984-08-14 Environmental Technology (U.S.), Inc. Recovery of metal from waste water by chemical precipitation
DE3308179A1 (de) * 1983-03-08 1984-11-29 Argentum Beck Und Gebhart Ohg Vorrichtung zum entgiften von oxidierbare organische und/oder anorganische substanzen enthaltende fluessigkeiten
US4579721A (en) * 1984-08-03 1986-04-01 Getty Oil Company Process for recovering metals from waste
US4680126A (en) * 1986-02-18 1987-07-14 Frankard James M Separation and recovery of reusable heavy metal hydroxides from metal finishing wastewaters

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Chemical Abstracts, Band 105, 1986, (Columbus, Ohio, US), siehe Seite 255 *
Chemical Abstracts, Band 92, 1980, (Columbus, Ohio, US), siehe Seite 239 *
Chemical Abstracts, Band 94, 1981, (Columbus, Ohio, US), M.Tels et al.: "Recovery of pure metal salts from mixed metal hydroxide sludges", siehe Seite 222 *
Chemical Abstracts, Band 94, 1981, Columbus, Ohio, US), siehe Seite 244 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6716403B2 (en) * 2000-11-14 2004-04-06 Japan Pionics Co., Ltd. Method of recovering a cleaning agent
US7297315B2 (en) 2000-11-14 2007-11-20 Japan Pionics Co., Ltd Method of recovering a cleaning agent
CN103014337A (zh) * 2013-01-10 2013-04-03 北京矿冶研究总院 一种酸浸溶液中铜、铬、锌的分离方法

Also Published As

Publication number Publication date
FI892164L (fi) 1989-05-05
DE3872870D1 (de) 1992-08-20
DK221289D0 (da) 1989-05-05
BR8807193A (pt) 1989-10-17
FI892164A7 (fi) 1989-05-05
JPH02501578A (ja) 1990-05-31
AU2321488A (en) 1989-04-17
DE3729913A1 (de) 1989-03-23
FI892164A0 (fi) 1989-05-05
KR890701781A (ko) 1989-12-21
DK221289A (da) 1989-07-05
AU609191B2 (en) 1991-04-26
EP0333796A1 (fr) 1989-09-27
ES2008025A6 (es) 1989-07-01
EP0333796B1 (fr) 1992-07-15
ATE78303T1 (de) 1992-08-15

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